title: Development and validation of automated SPE-LC-MS/MS method for determination of indapamide in human whole blood and its application to real study samples.
abstract: A fast and simple liquid chromatography-electrospray ionization tandem mass spectrometry method for determination of indapamide in human whole blood was developed and validated. The sample extraction of indapamide from human whole blood was achieved using automated solid-phase extraction. Chromatographic separation was performed on Kinetex C18 column (100 × 2.1 mm, 1.7 µm particle size) using acetonitrile and 2 mm ammonium formate in ratio 90:10 (v/v) as a mobile phase. The mass spectrometer was operated in the multiple reaction monitoring mode using positive electrospray ionization for indapamide and the internal standard (zolpidem tartarate). The total run time was 2.5 min. The present method was found to be linear in the concentration range of 1-50 ng/mL with the coefficient of determination 0.9987. The absolute recoveries of indapamide were 90.51-93.90%. The method was validated according the recommendations for validation of bioanalytical methods of European Medicines Agency guideline and was successfully used to analyze human whole blood samples for application in a pharmacokinetic study.
authors.affiliation: Faculty of Pharmacy, University of 'Ss Cyril and Methodius', Skopje, Republic of Macedonia.
authors.forename: N
authors.initials: N
authors.lastname: Nakov
authors.forename: K
authors.initials: K
authors.lastname: Mladenovska
authors.forename: N
authors.initials: N
authors.lastname: Labacevski
authors.forename: A
authors.initials: A
authors.lastname: Dimovski
authors.forename: R
authors.initials: R
authors.lastname: Petkovska
authors.forename: A
authors.initials: A
authors.lastname: Dimitrovska
authors.forename: Z
authors.initials: Z
authors.lastname: Kavrakovski
mesh_terms: D000328:Adult; D000959:Antihypertensive Agents / Q000097:blood* / Q000302:isolation & purification; D002853:Chromatography, Liquid / Q000379:methods*; D006801:Humans; D007190:Indapamide / Q000097:blood* / Q000302:isolation & purification; D057230:Limit of Detection; D008297:Male; D052616:Solid Phase Extraction / Q000379:methods*; D053719:Tandem Mass Spectrometry / Q000379:methods*
chemical_list: D000959:Antihypertensive Agents; D007190:Indapamide
keywords: LC-MS/MS; human whole blood; indapamide; pharmacokinetics